CN101376589A - Ferrite material and method for producing ferrite material - Google Patents
Ferrite material and method for producing ferrite material Download PDFInfo
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- CN101376589A CN101376589A CNA2008102105591A CN200810210559A CN101376589A CN 101376589 A CN101376589 A CN 101376589A CN A2008102105591 A CNA2008102105591 A CN A2008102105591A CN 200810210559 A CN200810210559 A CN 200810210559A CN 101376589 A CN101376589 A CN 101376589A
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Abstract
The invention relates to a ferrite material (ferrite sintered body, ferrite powders) having a composition formula of (1-x-y-z)(Li0.5Fe0.5)O.xZnO.y(Mn, Fe)2O3.zCuO, wherein x, y, z, and a satisfy 0.175<=x<=0.29; 0.475<=y<=0.51; 0.07<=z<=0.22; and 0.02<=a<=0.055 in a case of a=Mn/(Mn+Fe). At least one of Co oxide, Co hydroxide, and Co carbonate in an amount of 1 wt. % or less on the basis of CoO may be contained in 100 wt % of the ferrite material. The ferrite material has a normalized impedance ZN of 40000 Omega/m or more at 30 MHz and a normalized impedance ZN of 60000 Omega/m or more at 100 MHz as well as a specific resistance of 106 Omegam or more.
Description
Technical field
The present invention relates in high frequency band, have the Ferrite Material and the manufacture method thereof of high resistance.
Background technology
In the noise filter of the noise transmission that stops electronics, as the wave filter of the various prevention high-frequency band signals compositions transmission that propose to utilize, known have a noise filter of for example ferrite core being implemented coiling.
In these noise filters, the magnetoimpedance that utilizes Ferrite Material to have along with the miniaturization of in recent years various electronicss, requires to have the Ferrite Material of high resistance especially in high frequency band.
In the past, in noise filter, use the Ferrite Material of Mn-Zn class and Ni-Zn class.Mn-Zn class Ferrite Material is owing to having high permeability, so though the impedance in the kHz frequency band is big, because resistivity is little to about 1 Ω m, so increase because of the eddy current in the ferrite makes loss in the MHz frequency band.For this reason, in the frequency more than 10HMz, impedance reduces, and is difficult to use in the noise of removing in the above high frequency band of 30MHz.In addition, because resistivity is little,, except being increased in manufacturing processes such as inserting insulant between iron core and the coiling, also there is the problem that is difficult to miniaturization so be difficult to iron core is implemented directly coiling.
On the other hand, Ni-Zn class ferrite since resistivity greatly to 10
6More than the Ω m,, in the frequency more than 10MHz, can access than the high impedance of Mn-Zn class ferrite so the influence of eddy current losses is little.For this reason, the main Ni-Zn class ferrite that uses in the noise remove in the high frequency band more than 30MHz.In addition, because Ni-Zn class ferrite resistivity is big, can directly coiling on iron core so exist, advantage that also can miniaturization.
But, Ni-Zn class ferrite is because magnetostriction is big, and the variation of the magnetic properties that is caused by external stress is big, so for example after ferrite core is implemented coiling, in case implement resin cast in order to improve reliability, will have the problem that permeability is changed owing to this stress.In addition, be principal constituent owing to contain the Ni of high price, so the problem that also exists manufacturing cost to raise.
As the little material of Ni, magnetostriction that does not contain high price, known Li class Ferrite Material.For example, open the spy and to have proposed a kind of Li-Cu-Zn ferrite in the 2004-153197 communique, wherein by making material consist of Li
0.5xZn
ZCu
aFe
2+0.5x-yMn
yO
4(0.10＜x＜1.00,0.13＜y＜0.80,0＜z＜0.90,0.02＜a＜0.40,
), just can low-temperature sintering, realize the raising of resistivity thus.
Summary of the invention
But above-mentioned Li-Cu-Zn ferrite to be to use in stacked electronic part, can be purpose with the Ferrite Material of the low-temperature sintering type of silver-colored inner conductor roasting simultaneously, for desired impedance characteristic in the purposes such as noise filter but without any consideration.In addition, above-mentioned Li-Cu-Zn ferrite contains Mn as bioelement, but because the content of its Mn is many, so think opposite with the raising of resistivity, initial permeability descends, and corresponding therewith, impedance also descends.
Like this, in Li class ferrite in the past, also do not propose to be suitable for Ferrite Materials purposes, that in high frequency band, have high resistance such as noise filter.
The objective of the invention is to, a kind of Ferrite Material is provided, it has in the high resistance in high frequency band, also have and to implement the directly high resistivity of coiling to iron core, and the variation of the magnetic properties that is caused by external stress is little, the core material that can provide, be used for winding parts such as noise filter and reactance coil at an easy rate or wave absorber etc.
In addition, another object of the present invention is to, provide a kind of can high precision, make the Ferrite Material manufacture method of above-mentioned such Ferrite Material (ferrite cemented body, ferrite powder) simply.
The present inventor to achieve these goals, the ferritic composition of Li class is studied with keeping on improving, found that, in the Li-Zn-Mn-Cu ferrite, contain more Cu by making it, simultaneously the Mn amount is limited in the specified range, just can access such Ferrite Material, its magnetostriction is little, do not use Ni and realize low price, keep the ferritic inherent feature of Li class, have high impedance in the frequency band more than 30MHz simultaneously, and resistivity is 10
6More than the Ω m.
And the present inventor finds, by with respect to above-mentioned Ferrite Material, contains at least a in Co oxide compound, Co oxyhydroxide, the Co oxycarbide slightly, can further improve the impedance in the above frequency band of 30MHz.
Ferrite Material of the present invention, its composition formula are (1-x-y-z) (Li
0.5Fe
0.5) OxZnOy (Mn, Fe)
2O
3ZCuO, and under the situation of a=Mn/ (Mn+Fe), x, y, z, a satisfy 0.175 ≦ x ≦ 0.29,0.475 ≦ y ≦ 0.51,0.07 ≦ z ≦ 0.22,0.02 ≦ a ≦ 0.055.
Ferrite Material of the present invention with respect to above-mentioned Ferrite Material 100 quality %, as additive, is pressed CoO and is converted, and contains at least a in the following Co oxide compound of 1 quality %, Co oxyhydroxide, the Co oxycarbide.
Ferrite Material of the present invention is: in having the Ferrite Material of said structure, and the normalized impedance Z under 30MHz
NBe the above and normalized impedance Z under 100MHz of 40000 Ω/m
NBe 60000 Ω/more than the m.
Ferrite Material of the present invention is: in having the Ferrite Material of said structure, resistivity is 10
6More than the Ω m.
Ferrite Material of the present invention is: in having the Ferrite Material of said structure, the velocity of variation of the initial permeability when pressurizeing under the pressure of 30MPa is in ± 10%.
Ferrite Material of the present invention can be following mode: each handles the ferrite cemented body that obtains successively raw material powder to be implemented calcining, pulverizing, moulding and roasting; The ferrite powder that the roasting raw material powder obtains; Each handles the ferrite powder that obtains successively raw material powder to be implemented calcining, pulverizing and roasting; Successively raw material powder is implemented calcining, pulverizing, moulding, roasting and pulverize each and handle the ferrite powder that obtains etc.The median size of ferrite powder suitably selects a few μ m to hundreds of μ m according to application target.
The method of making Ferrite Material of the present invention (ferrite cemented body) comprises: the operation of preparation raw material powder, the composition formula of this raw material powder is (1-x-y-z) (Li
0.5Fe
0.5) OxZnOy (Mn, Fe)
2O
3ZCuO, and under the situation of a=Mn/ (Mn+Fe), x, y, z, a satisfy 0.175 ≦ x ≦ 0.29,0.475 ≦ y ≦ 0.51,0.07 ≦ z ≦ 0.22,0.02 ≦ a ≦ 0.055; The calcining raw materials powder obtains calcining the operation of powder; Pulverize the operation that the calcining powder obtains comminuted powder; The shaping powder flour obtains the operation of formed body; Obtain the operation of ferrite cemented body with the roasting formed body.
The method of making Ferrite Material of the present invention (ferrite powder) can comprise: the operation of preparation raw material powder, the composition formula of this raw material powder is (1-x-y-z) (Li
0.5Fe
0.5) OxZnOy (Mn, Fe)
2O
3ZCuO, and under the situation of a=Mn/ (Mn+Fe), x, y, z, a satisfy 0.175 ≦ x ≦ 0.29,0.475 ≦ y ≦ 0.51,0.07 ≦ z ≦ 0.22,0.02 ≦ a ≦ 0.055; The roasting raw material powder obtains the operation of ferrite powder.Temperature during roasting is preferably 800～1050 ℃.In the operation of preparation raw material powder with carry out also can having pair raw material powder to carry out the operation of granulation between the operation of roasting.
The method of making Ferrite Material of the present invention (ferrite powder) can comprise: the operation of preparation raw material powder, the composition formula of this raw material powder is (1-x-y-z) (Li
0.5Fe
0.5) OxZnOy (Mn, Fe)
2O
3ZCuO, and under the situation of a=Mn/ (Mn+Fe), x, y, z, a satisfy 0.175 ≦ x ≦ 0.29,0.475 ≦ y ≦ 0.51,0.07 ≦ z ≦ 0.22,0.02 ≦ a ≦ 0.055; The calcining raw materials powder obtains calcining the operation of powder; Pulverize the operation that the calcining powder obtains comminuted powder; Obtain the operation of ferrite powder with the roasting comminuted powder.In the operation of pulverizing the calcining powder with carry out also can having pair comminuted powder to carry out the operation of granulation between the operation of roasting.
The method of making Ferrite Material of the present invention (ferrite powder) can comprise: the operation of preparation raw material powder, the composition formula of this raw material powder is (1-x-y-z) (Li
0.5Fe
0.5) OxZnOy (Mn, Fe)
2O
3ZCuO, and under the situation of a=Mn/ (Mn+Fe), x, y, z, a satisfy 0.175 ≦ x ≦ 0.29,0.475 ≦ y ≦ 0.51,0.07 ≦ z ≦ 0.22,0.02 ≦ a ≦ 0.055; The calcining raw materials powder obtains calcining the operation of powder; Pulverize the operation that the calcining powder obtains comminuted powder; The shaping powder flour obtains the operation of formed body; The roasting formed body obtains the operation of sintered compact; With pulverize the operation that sintered compact obtains ferrite powder.
The method of making Ferrite Material of the present invention (ferrite cemented body, ferrite powder) also can comprise: during before carry out above-mentioned roasting, interpolation is with respect to being added material 100 quality %, press CoO and convert, at least a operation in the Co oxide compound below the 1 quality %, Co oxyhydroxide, the Co oxycarbide.
According to the present invention, can access a kind of Ferrite Material (ferrite cemented body, ferrite powder), its normalized impedance Z under 30MHz
NBe the above and normalized impedance Z under 100MHz of 40000 Ω/m
NBe to have high impedance in the above such high frequency band of 60000 Ω/m.By the core material of this ferrite cemented body as winding parts such as noise filter and reactance coils used, just can be provided at the noise filter that can efficiently stop the transmission of noise in the high frequency band.
In addition, according to the present invention, can access and have 10
6The Ferrite Material (ferrite cemented body, ferrite powder) of the high resistivity that Ω m is above.By the core material of this ferrite cemented body as winding parts such as noise filter and reactance coils used, owing to can implement directly coiling, just can reduce the operation of insertion insulant etc. to iron core, can realize the miniaturization of winding part simultaneously.
And, according to the present invention, since obtain magnetostriction little, with respect to the little Ferrite Material of the velocity of variation of external stress magnetic properties (ferrite cemented body, ferrite powder), so the core material of winding parts such as noise filter by this ferrite cemented body being used to need resin cast and reactance coil just can reduce the deviation of magnetic properties.
And, according to Ferrite Material of the present invention (ferrite cemented body, ferrite powder), owing to do not contain the Ni of high price, so can realize the reduction of manufacturing cost, as the core material of winding parts such as noise filter and reactance coil, can provide preferred ferrite cemented body at an easy rate.
In addition, be distributed in the resin etc. and moulding, just can be provided at the wave absorber that has good electric wave absorptive character in the high frequency band at an easy rate by making ferrite powder according to the present invention.
Description of drawings
Fig. 1 be the expression embodiment 1 suitable example/comparative example in composition and the chart of characteristic;
Fig. 2 be the expression embodiment 2 suitable example/comparative example in composition and the chart of characteristic;
Fig. 3 be the expression embodiment 3 suitable example/comparative example in composition and the chart of characteristic;
Fig. 4 be the expression embodiment 4 suitable example/comparative example in composition and the chart of characteristic; And
Fig. 5 be the expression embodiment 5 suitable example/comparative example in composition and the chart of characteristic.
Preferred implementation
The composition that Ferrite Material among the present invention is described in detail in detail below limits reason.
At composition formula (1-x-y-z) (Li
0.5Fe
0.5) OxZnOy (Mn, Fe)
2O
3Among the zCuO, x is the containing ratio of ZnO, preferred 0.175～0.29 (more than 0.175, below 0.29 ,～the meaning following identical) scope.Be lower than at 0.175 o'clock, initial permeability diminishes, the normalized impedance Z under the 30MHz
NBe lower than 40000 Ω/m, when surpassing 0.29, though the normalized impedance Z under the 30MHz
NSurpass 40000 Ω/m, but the normalized impedance ZN under the 100MHz is lower than 60000 Ω/m, Curie temperature is low simultaneously, so be not preferred.
Y is Fe
2O
3Suitable containing ratio, be to remove (Li
0.5Fe
0.5) containing ratio beyond the Fe among the O, preferred 0.475～0.51 scope.Be lower than at 0.475 o'clock, because the normalized impedance Z under 30MHz and the 100MHz
NLow, so be not preferred; When surpassing 0.51, because the normalized impedance Z under 30MHz and the 100MHz
NAll low, and resistivity is lower than 10
6Ω m is not so be preferred.Preferred scope is 0.49～0.51。(Li is arranged again
0.5Fe
0.5) containing ratio of O is surplus portion except that above-mentioned x and y and z described later.
By using Mn
2O
3Replace above-mentioned Fe
2O
3A part, just can improve the normalized impedance Z under 30MHz and the 100MHz
NUnder the situation of a=Mn/ (Mn+Fe), the scope of a preferred 0.02～0.055.Be lower than at 0.02 o'clock, do not having normalized impedance Z
NThe raising effect, when surpassing 0.055, because the normalized impedance Z under the 30MHz
NBe lower than 40000 Ω/m, and resistivity is lower than 10
6Ω m is not so be preferred.
With this Mn
2O
3Containing ratio to be defined in the above-mentioned scope be one of feature of the present invention.About this point, (13mol%～80mol%) so initial permeability descends, correspondingly, thinks normalized impedance Z because the ferritic Mn content of Li-Cu-Zn of opening the 2004-153197 communique according to the described spy of background technology usually mostly is 0.13～0.80
NAlso descend, be not suitable as the core material use of winding parts such as noise filter.Have again, convert as the general expression of opening the 2004-153197 communique by the spy, then the Mn among the present invention
2O
3Containing ratio be (12.62mol% is following) below 0.1262.
In above-mentioned composition formula, z is the containing ratio of CuO, is preferably 0.07～0.22 scope.Containing this CuO more is principal character of the present invention.CuO replaces (Li
0.5Fe
0.5) material of a part of O, owing to contain the CuO of above-mentioned scope, just can improve normalized impedance Z widely
N, can take into account the normalized impedance Z that reaches under the 30MHz
NBe the normalized impedance Z more than 40000 Ω/m, under the 100MHz
NIt is the above effect of 60000 Ω/m.Z is being lower than at 0.07 o'clock, does not have normalized impedance Z
NThe raising effect, when surpassing 0.22, the normalized impedance Z under the 30MHz
NBe lower than 40000 Ω/m, so be not preferred.Preferred scope is 0.10～0.19.
Limit reason owing to satisfy above-mentioned composition, just can access the normalized impedance Z that takes into account under the 30MHz
NBe the normalized impedance Z more than 40000 Ω/m, under the 100MHz
NBe that 60000 Ω/more than the m, resistivity is 10 simultaneously
6More than the Ω m, and the velocity of variation of the initial permeability when pressurizeing with pressure 30MPa is ± 10% with interior Ferrite Material.
And the Ferrite Material that will have above-mentioned composition is as 100 quality %, contains at least a in Co oxide compound below the 1 quality %, Co oxyhydroxide, the Co oxycarbide by converting by CoO, just can further improve the normalized impedance Z in the high frequency band
NIn case content is pressed CoO and converted when surpassing 1 quality %, the magnetostriction of material will become greatly, because of the variation change of external stress magnetic properties is big, and the normalized impedance Z under while 30MHz and the 100MHz
NDescend, so be not preferred.
As Ferrite Material of the present invention with such composition, have following mode: each handles the ferrite cemented body that obtains successively raw material powder to be implemented calcining, pulverizing, moulding and roasting, perhaps, the ferrite powder that obtains by raw material powder by the whole bag of tricks as described below.For example, as the core material of winding parts such as noise filter and reactance coil, can use ferrite cemented body.In addition, be distributed in the resin etc. by making ferrite powder, the shape moulding with predetermined just can be produced on the wave absorber that has good electric wave absorptive character in the high frequency band.Have, ferritic median size of the present invention according to the purposes of using, can suitably select a few μ m to hundreds of μ m again.The dispersiveness of consideration in resin etc., operability etc., the powder that preferable particle size difference is little.
The manufacture method of Ferrite Material of the present invention (ferrite cemented body, ferrite powder) will be described below.At first, set forth the manufacture method of ferrite cemented body.
Preparing composition formula is (1-x-y-z) (Li
0.5Fe
0.5) OxZnOy (Mn, Fe)
2O
3ZCuO, and a=Mn/ (Mn+Fe), x, y, z, a satisfy 0.175 ≦ x ≦ 0.29,0.475 ≦ y ≦ 0.51,0.07 the material of ≦ z ≦ 0.22,0.02 ≦ a ≦ 0.055 is perhaps with respect to this material (being added material) 100 quality %, press CoO as additive and convert, contain at least a material in the following Co oxide compound of 1 quality %, Co oxyhydroxide, the Co oxycarbide.
Can be in the operation that before calcining process described later, is prepared above-mentioned materials.That is, also can in each operation before weighing, mixing, calcining, pulverizing, moulding, prepare above-mentioned materials.For example, weighing at first, mixing and calcining are as the carbonate powder and the oxide powder of the starting materials of all elements; Can first weighing, mix other raw material powder except that raw material powders such as Li and Co, after calcining, raw material powders such as Li and Co are mixed into this calcining powder (being added material) after, pulverize, moulding.Perhaps, can also the comminuted powder (being added material) after being mixed into pulverizing after, carry out roasting.
In calcination process, 800 ℃～900 ℃ of preferred calcination temperature.Calcination time is preferably 2 hours～and 5 hours.In addition, calcination atmosphere is preferably in the atmosphere or in the oxygen atmosphere.
In pulverizing process, preferably in pure water or ethanol, pulverize.In addition, the median size of the comminuted powder after the pulverizing is preferably 0.5 μ m～1.5 μ m.
By the comminuted powder after the desirable moulding means moulding pulverizing.Can before moulding, carry out granulation with prilling granulator to comminuted powder as required.Forming pressure is preferably 70MPa～150MPa.
The formed body that roasting obtains by the way obtains ferrite cemented body of the present invention.Preferred 950 ℃～1050 ℃ of maturing temperature.Preferred 2～5 hours of roasting time.In addition, calcination atmosphere is preferably in atmosphere or in the oxygen atmosphere.
The manufacture method of ferrite powder then, is described.As the method for making ferrite powder, exist and implement 5 kinds of method for makings that each program as described below obtains ferrite powder successively.
Preparation → the roasting of (method for making a1) raw material powder
(method for making a2) raw material powder preparation → granulation → roasting
(method for making b1) raw material powder preparation → calcining → pulverizing → roasting
(method for making b2) raw material powder preparation → calcining → pulverizing → granulation → roasting
(method for making c) raw material powder preparation → calcining → pulverizing → moulding → roasting → pulverizing
Method for making a1 is behind raw material powders such as weighing, mixed carbonate powder and oxide powder, with 800 ℃～1050 ℃ methods of carrying out roasting.Method for making a2 is behind weighing, mixing raw material powder, through granulation, again with 800 ℃～1050 ℃ methods of carrying out roasting.In method for making a1, a2, maturing temperature is made as 800 ℃～1050 ℃ the reasons are as follows.
When maturing temperature is lower than 800 ℃, because solid state reaction does not generate the ferrite phase,, then cause grain growing in case surpass 1050 ℃, condense, so be not preferred.In method for making a1, a2, b1, b2, can also pulverize the powder after the roasting.In method for making a1, a2, because the shrinking percentage when comparing roasting with other method for making is big, so obtain the powder of smaller particle diameter easily.In addition, because the physical strength of powder is also lower, so can access thinner particle diameter by pulverizing.
Method for making b1 is the powder that weighing, raw materials mixed powder are obtained through calcining, pulverizing, still with 950 ℃～1050 ℃ methods of carrying out roasting.Method for making b2 is from weighing, raw materials mixed powder obtain prilling powder through the powder of calcining, pulverizing after, still with 950 ℃～1050 ℃ methods of carrying out roasting.In method for making b1, b2, owing to compare with the situation of method for making a1, a2, the shrinking percentage during roasting is little, so obtain the powder of bigger particle diameter easily.In addition, because roasting calcining powder so the deviation of the composition that powder is mutual, powder is interior is little, obtains the powder of homogeneous easily.In addition, can easily make roughly spheric powder about particle diameter 50 μ m～100 μ m.
Method for making c is after making ferrite cemented body by aforesaid program, pulverizes the method for this ferrite cemented body.In method for making c, compare with the situation of other method for making, can access the powder of big particle diameter.Yet, in pulverizing process,, remove micro mist so preferably carry out stage treatment owing to do not avoid the generation of micro mist.
Even if in the manufacturing of ferrite powder, also identical with the manufacturing of ferrite cemented body, preferably with respect to being added material 100 quality %, as additive, press CoO and convert, add at least a kind in the following Co oxide compound of 1 quality %, Co oxyhydroxide, the Co oxycarbide.In the case, the operation of adding Co can be carried out before calcining process.That is for example, can in above-mentioned method for making a1～c, be (1-x-y-z) (Li, at composition formula
0.5Fe
0.5) OxZnOy (Mn, Fe)
2O
3Co is added in being added of zCuO in the material, the preparation raw material powder.In addition, in method for making b1, b2, c, also can first weighing, mix other raw material powder except that Co and calcine after, interpolation Co pulverizes then in calcining powder (being added material).Perhaps, roasting again after adding in also can the comminuted powder (being added material) after pulverizing.
(embodiment 1)
Final composition becomes various compositions shown in Figure 1 (for (Li
0.5Fe
0.5) O, ZnO, (Mn, Fe)
2O
3, CuO mol% mark.0.01 of x, y, z is equivalent to 1mol% in the composition formula) like that, weighing, the carbonate powder that is mixed into starting materials and oxide powder were calcined 3 hours with 900 ℃ in atmosphere.The calcining powder that utilizes the ball mill case of wet attrition to obtain carries out drying after making it become the size of 1.5 μ m from 0.5 μ m.
In the powder that obtains, add the polyvinyl alcohol of 1 quality %, carry out granulation and become the granulation powder, with forming pressure 150MPa, this granulation powder is shaped to the ring-type of external diameter 9mm * internal diameter 4mm * thick 3mm, long limit 20mm * minor face 10mm * thick 5mm's is tabular, with the frame shape of housing 9.5mm * inside casing 4.7mm * thick 2.4mm, in atmosphere with 1000 ℃ with the formed body roasting that obtains 3 hours, obtain Ferrite Material.
The ring-type Ferrite Material that obtains is implemented coiling, utilize LCR instrument (HEWLETTPACKARD makes, device name 4285A) to measure initial permeability μ with f=100kHz, H=0.4A/m
iMeasuring result is shown in Fig. 1.
In addition, the use electric impedance analyzer (Agilent makes, E4991A, Off イ Network ス チ ャ-16454A), with OSC level 100mV, relative permeability μ ', the μ of the ring-type Ferrite Material that under f=1MHz～1GHz, measures ", use following formula (1) to calculate normalized impedance Z
NNormalized impedance Z under 30MHz and 100MHz
NThe results are shown in Fig. 1.Have, in following formula (1), f is a frequency, μ again
0Be the permeability of vacuum, μ ' is the relative permeability (real part) of material, μ " be the relative permeability (imaginary part) of material.
Z
N＝2πfμ
0(μ’
2+μ”
2)
1/2 (1)
In addition, from the tabular Ferrite Material that obtains, cut out the test portion of long limit 17mm * minor face 2mm * thick 2mm,, utilize the two-terminal method to measure the resistance of test portion at two ends coating electrically conductive paste.Measuring result is shown in Fig. 1.
And, the Ferrite Material of the picture frame shape that obtains is implemented coiling, by a 30MPa pressurization, with the initial permeability μ of LCR apparatus measures pressurization front and back same as described above
i, obtain initial permeability μ
iVelocity of variation.Measuring result is shown in Fig. 1.Have, in Fig. 1, the test portion numbering of band * mark is a comparative example again, and what do not have the * mark is to be fit to example (embodiments of the invention).Should
*Be marked at same meaning among other Fig. 2～Fig. 5 described later.
As by as indicated in Fig. 1, be (1-x-y-z) (Li at composition formula as can be known
0.5Fe
0.5) OxZnOy (Mn, Fe)
2O
3ZCuO in the Ferrite Material of a=Mn/ (Mn+Fe), can access containing ratio at ZnO and is in 0.175～0.29 the scope, takes into account the normalized impedance Z at 30MHz place
NBe that 40000 Ω/m is above, the normalized impedance Z at 100MHz place
NBe 60000 Ω/more than the m, and satisfy resistivity 10
6The Ferrite Material that Ω m is above.In addition, as by μ
iVelocity of variation is indicated, can access the initial permeability Ferrite Material little with respect to the velocity of variation of external stress as can be known.
(embodiment 2)
Except that final composition uses various compositions shown in Figure 2, carry out the experiment identical with embodiment 1.It the results are shown in Fig. 2.
As by as indicated in Fig. 2, be (1-x-y-z) (Li at composition formula as can be known
0.5Fe
0.5) OxZnOy (Mn, Fe)
2O
3ZCuO in the Ferrite Material of a=Mn/ (Mn+Fe), can access at Fe
2O
3Containing ratio be in 0.475～0.51 the scope, take into account the normalized impedance Z at 30MHz place
NBe that 40000 Ω/m is above, the normalized impedance Z at 100MHz place
NBe 60000 Ω/more than the m, and satisfy resistivity 10
6The Ferrite Material that Ω m is above.In addition, as by μ
iVelocity of variation is indicated, can access the initial permeability Ferrite Material little with respect to the velocity of variation of external stress as can be known.
(embodiment 3)
Except that final composition uses various compositions shown in Figure 3, carry out the experiment identical with embodiment 1.It the results are shown in Fig. 3.
As indicated in Fig. 3, be (1-x-y-z) (Li at composition formula as can be known
0.5Fe
0.5) OxZnOy (Mn, Fe)
2O
3ZCuO in the Ferrite Material of a=Mn/ (Mn+Fe), can access containing ratio at CuO and is in 0.07～0.22 the scope, takes into account the normalized impedance Z at 30MHz place
NBe that 40000 Ω/m is above, the normalized impedance Z at 100MHz place
NBe 60000 Ω/more than the m, and satisfy resistivity 10
6The Ferrite Material that Ω m is above.In addition, as μ
iVelocity of variation is indicated, can access the initial permeability Ferrite Material little with respect to the velocity of variation of external stress as can be known.
(embodiment 4)
Except that final composition uses various compositions shown in Figure 4, carry out the experiment identical with embodiment 1.It the results are shown in Fig. 4.
As by as indicated in Fig. 4, be (1-x-y-z) (Li at composition formula as can be known
0.5Fe
0.5) OxZnOy (Mn, Fe)
2O
3ZCuO in the Ferrite Material of a=Mn/ (Mn+Fe), can access containing ratio at (Mn/ (Mn+Fe)) and is in 0.02～0.055 the scope, takes into account the normalized impedance Z at 30MHz place
NBe that 40000 Ω/m is above, the normalized impedance Z at 100MHz place
NBe 60000 Ω/more than the m, and satisfy resistivity 10
6The Ferrite Material that Ω m is above.In addition, as by μ
iVelocity of variation is indicated, can access the initial permeability Ferrite Material little with respect to the velocity of variation of external stress as can be known.
(embodiment 5)
Remove final composition principal constituent shown in Figure 5 is formed as 100 quality %, and by CoO conversion interpolation Co of amount shown in Figure 5
3O
4Outside addition, carry out the experiment identical with embodiment 1.It the results are shown in Fig. 5.
As by as indicated in Fig. 5, be (1-x-y-z) (Li with respect to composition formula as can be known
0.5Fe
0.5) OxZnOy (Mn, Fe)
2O
3ZCuO, Ferrite Material 100 quality 100% of a=Mn/ (Mn+Fe) contain the Co oxide compound of the following addition of 1 quality % by converting by CoO, make the normalized impedance Z at 30MHz and 100MHz place
NImprove.In addition, as can be known owing to containing CoO, so resistivity satisfies 10
6More than the Ω m, μ
iVelocity of variation is also little.
(embodiment 6)
The granulation powder that not moulding is made according to embodiment 1, and in atmosphere with 1000 ℃ of roastings 3 hours, obtain the roughly globular Ferrite Material (ferrite powder) of median size 75 μ m.The manufacture method of this ferrite powder is equivalent to above-mentioned method for making b2.The ferrite powder 90 quality % and thermoplastic resin 10 quality 10% that obtain are mixed, in resin, disperse ferrite powder equably, after heating in order to improve resin flow, stirring, the moulding cool to room temperature, thus, produce tabular wave absorber.The electric wave absorptive character of the wave absorber that measurement is produced, result show to have good electric wave absorptive character in high frequency band.
Have again, identical with embodiment 6, make the ferrite powder that produces according to above-mentioned method for making except that method for making b2 disperse into to produce wave absorber in the thermoplastic resin, even if in this wave absorber, can confirm that also it has good electric wave absorptive character.
According to Ferrite Material of the present invention, in high frequency band, have in the high impedance, also have and to implement the directly high resistivity of coiling to iron core, and the variation of the magnetic properties that causes because of external stress is little, can provide at an easy rate, be suitable for the core material of winding parts such as noise filter and reactance coil or wave absorber etc. most.
Claims (15)
1. Ferrite Material, its composition formula is (1-x-y-z) (Li
0.5Fe
0.5) OxZnOy (Mn, Fe)
2O
3ZCuO is characterized in that,
Under the situation of a=Mn/ (Mn+Fe), x, y, z, a satisfy 0.175 ≦ x ≦ 0.29,0.475 ≦ y ≦ 0.51,0.07 ≦ z ≦ 0.22,0.02 ≦ a ≦ 0.055.
2. Ferrite Material according to claim 1 is characterized in that,
With respect to Ferrite Material 100 quality %, press CoO and convert, contain at least a in the following Co oxide compound of 1 quality %, Co oxyhydroxide, the Co oxycarbide.
3. Ferrite Material according to claim 1 and 2 is characterized in that,
Normalized impedance ZN under 30MHz is that the normalized impedance ZN of 40000 Ω/more than the m and under 100MHz is 60000 Ω/more than the m.
4. Ferrite Material according to claim 1 and 2 is characterized in that,
Resistivity is 10
6More than the Ω m.
5. Ferrite Material according to claim 1 and 2 is characterized in that,
The velocity of variation of the initial permeability when pressurizeing under the pressure of 30MPa is in ± 10%.
6. Ferrite Material according to claim 1 and 2 is characterized in that,
Described Ferrite Material be to raw material powder implement successively to calcine, pulverizing, moulding and roasting each handle the ferrite cemented body that obtains.
7. Ferrite Material according to claim 1 and 2 is characterized in that,
Described Ferrite Material is the ferrite powder that the roasting raw material powder obtains.
8. Ferrite Material according to claim 1 and 2 is characterized in that,
Described Ferrite Material be to raw material powder implement successively to calcine, pulverizing and roasting each handle the ferrite powder that obtains.
9. Ferrite Material according to claim 1 and 2 is characterized in that,
Described Ferrite Material be to raw material powder implement successively to calcine, pulverizing, moulding, roasting and pulverize each and handle the ferrite powder that obtains.
10. method for manufacturing ferrite material may further comprise the steps:
The preparation raw material powder, the composition formula of described raw material powder is (1-x-y-z) (Li
0.5Fe
0.5) OxZnOy (Mn, Fe)
2O
3ZCuO, and under the situation of a=Mn/ (Mn+Fe), x, y, z, a satisfy 0.175 ≦ x ≦ 0.29,0.475 ≦ y ≦ 0.51,0.07 ≦ z ≦ 0.22,0.02 ≦ a ≦ 0.055;
The calcining raw materials powder obtains calcining powder;
Pulverize the calcining powder and obtain comminuted powder;
The shaping powder flour obtains formed body; With
The roasting formed body obtains ferrite cemented body.
11. method for manufacturing ferrite material may further comprise the steps:
The preparation raw material powder, the composition formula of described raw material powder is (1-x-y-z) (Li
0.5Fe
0.5) OxZnOy (Mn, Fe)
2O
3ZCuO, and under the situation of a=Mn/ (Mn+Fe), x, y, z, a satisfy 0.175 ≦ x ≦ 0.29,0.475 ≦ y ≦ 0.51,0.07 ≦ z ≦ 0.22,0.02 ≦ a ≦ 0.055; With
The roasting raw material powder obtains ferrite powder.
12. method for manufacturing ferrite material according to claim 11 is characterized in that,
Temperature during the described raw material powder of roasting is 800 ℃～1050 ℃.
13. method for manufacturing ferrite material may further comprise the steps:
The preparation raw material powder, the composition formula of described raw material powder is (1-x-y-z) (Li
0.5Fe
0.5) OxZnOy (Mn, Fe)
2O
3ZCuO, and under the situation of a=Mn/ (Mn+Fe), x, y, z, a satisfy 0.175 ≦ x ≦ 0.29,0.475 ≦ y ≦ 0.51,0.07 ≦ z ≦ 0.22,0.02 ≦ a ≦ 0.055;
The calcining raw materials powder obtains calcining powder;
Pulverize the calcining powder and obtain comminuted powder; With
The roasting comminuted powder obtains ferrite powder.
14. a method for manufacturing ferrite material may further comprise the steps:
The preparation raw material powder, the composition formula of described raw material powder is (1-x-y-z) (Li
0.5Fe
0.5) OxZnOy (Mn, Fe)
2O
3ZCuO, and under the situation of a=Mn/ (Mn+Fe), x, y, z, a satisfy 0.175 ≦ x ≦ 0.29,0.475 ≦ y ≦ 0.51,0.07 ≦ z ≦ 0.22,0.02 ≦ a ≦ 0.055;
The calcining raw materials powder obtains calcining powder;
Pulverize the calcining powder and obtain comminuted powder;
The shaping powder flour obtains formed body;
The roasting formed body obtains sintered compact; With
Pulverize sintered compact and obtain ferrite powder.
15., further comprising the steps of according to the described method for manufacturing ferrite material of arbitrary claim in the claim 10～14:
During before carry out described roasting, with respect to being added material 100 quality %, pressing CoO and convert, add at least a in the following Co oxide compound of 1 quality %, Co oxyhydroxide, the Co oxycarbide.
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| JP2008-208663 | 2008-08-13 | ||
| JP2008208663A JP5549063B2 (en) | 2007-08-31 | 2008-08-13 | Ferrite material and method for producing ferrite material |
| JP2008208663 | 2008-08-13 |
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| CN106219610A (en) * | 2016-07-02 | 2016-12-14 | 宁波江东索雷斯电子科技有限公司 | A kind of preparation method of Conjugate ferrite nano magnetic material |
| CN112017841A (en) * | 2020-08-28 | 2020-12-01 | 中钢天源股份有限公司 | Multi-pole magnetic ring and manufacturing method thereof |
Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| WO2010125626A1 (en) * | 2009-04-27 | 2010-11-04 | 株式会社リケン | Electromagnetic absorber for anechoic chamber |
| JP7484086B2 (en) | 2019-05-15 | 2024-05-16 | 株式会社プロテリアル | Manufacturing method of MnZn ferrite core |
| CN113192717B (en) * | 2021-04-22 | 2023-06-30 | 兰州大学 | Metal soft magnetic composite material and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| JPS6076107A (en) * | 1983-09-12 | 1985-04-30 | エヌ・ベ−・フイリツプス・フル−イランペンフアブリケン | Magnetic core based on lithium-zinc-manganese ferrite and method of producing same |
| JPS61205627A (en) * | 1985-03-09 | 1986-09-11 | Toda Kogyo Corp | Production of powder for electric wave absorber |
| JPH0653024A (en) * | 1991-07-26 | 1994-02-25 | Tokin Corp | Oxide magnetic powder, oxide nonmagnetic powder and magnetic bar code |
| DE69516664T2 (en) * | 1994-09-14 | 2001-01-11 | Koninkl Philips Electronics Nv | SINDERED MOLDED BODY, TRANSFORMER CORE AND INDUCTOR MADE OF LI (NI) ZN-FERRITE MATERIAL AND APPLICATIONS THEREOF |
| JP3246838B2 (en) * | 1994-09-30 | 2002-01-15 | 太陽誘電株式会社 | Oxide magnetic material |
| JP2004153197A (en) * | 2002-11-01 | 2004-05-27 | Koa Corp | Magnetic material and its producing process |
| JP2004153196A (en) * | 2002-11-01 | 2004-05-27 | Koa Corp | Magnetic material and its producing process |
| JP2005053759A (en) * | 2003-08-07 | 2005-03-03 | Koa Corp | Ferrite sintered compact and multilayer ferrite component using the same |
| TWI303073B (en) * | 2003-09-03 | 2008-11-11 | Tdk Corp | Ferrite material, ferrite sintered body, and inductor |
| JP4761187B2 (en) * | 2005-03-31 | 2011-08-31 | 日立金属株式会社 | Magnetic oxide material |
| WO2007032338A1 (en) * | 2005-09-13 | 2007-03-22 | Hitachi Metals, Ltd. | Ferrite material |
| JP2007076964A (en) * | 2005-09-15 | 2007-03-29 | Koa Corp | Magnetic material, and method for producing magnetic material |
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| CN106219610A (en) * | 2016-07-02 | 2016-12-14 | 宁波江东索雷斯电子科技有限公司 | A kind of preparation method of Conjugate ferrite nano magnetic material |
| CN106219610B (en) * | 2016-07-02 | 2017-09-01 | 烟台鑫洋电子有限公司 | A kind of preparation method of Conjugate ferrite nano magnetic material |
| CN112017841A (en) * | 2020-08-28 | 2020-12-01 | 中钢天源股份有限公司 | Multi-pole magnetic ring and manufacturing method thereof |
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| JP2009073724A (en) | 2009-04-09 |
| JP5549063B2 (en) | 2014-07-16 |
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